# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1594 # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95) data_global _publ_contact_author ; Dr Ulrich Fl\"orke Anorganische und Analytische Chemie Universit\"at-GH Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; _publ_contact_author_email uf@chemie.uni-paderborn.de _publ_contact_author_fax '+49 5251 60 3423' _publ_contact_author_phone '+49 5251 60 2496' _publ_contact_letter ; Please find below 4 data set(s) for strutures 2c, 2g, 5a, 5b in CIF format. These refer to our requested publication in Dalton Trans. Thank you very much! ; _publ_section_title ; The reaction of 2,6-Re~2~(CO)~8~(MeCN)~2~ with thiols. Formation of hydrido sulfido bridged dirhenium cluster complexes Re~2~(\m-H)(\m-SR)(CO)~8~ (R = H, n-Bu, Cy, Ph, p-C~6~H~4~F, C~6~F~5~, 2-naphtyl). ; loop_ _publ_author_name _publ_author_address 'Egold, Hans' ;Fachbereich Chemie und Chemietechnik Universit\"at-GH Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Schwarze, Detlef' ;Fachbereich Chemie und Chemietechnik Universit\"at-GH Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Fl\"orke, Ulrich' ;Fachbereich Chemie und Chemietechnik Universit\"at-GH Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; data_2c _audit_creation_method SHELXL-97 _chemical_formula_sum 'C14 H12 O8 Re2 S' _chemical_formula_weight 712.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.399(2) _cell_length_b 11.555(3) _cell_length_c 16.244(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.63(2) _cell_angle_gamma 90.00 _cell_volume 1929.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 6 _cell_measurement_theta_max 21 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.453 _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 12.677 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.359 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS P4' _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% 10 _diffrn_reflns_number 4567 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4434 _reflns_number_gt 3130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00304(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4434 _refine_ls_number_parameters 230 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.11189(4) 0.37027(4) 0.29320(2) 0.03591(14) Uani 1 1 d D . . Re2 Re 0.15889(4) 0.24069(3) 0.46168(3) 0.03873(15) Uani 1 1 d D . . S1 S 0.2778(2) 0.2225(2) 0.34175(16) 0.0375(6) Uani 1 1 d . . . C1 C 0.1566(11) 0.4003(10) 0.1827(8) 0.049(3) Uani 1 1 d . . . O1 O 0.1819(11) 0.4173(9) 0.1190(6) 0.083(3) Uani 1 1 d . . . C2 C -0.0386(11) 0.4722(10) 0.2793(7) 0.048(3) Uani 1 1 d . . . O2 O -0.1263(8) 0.5327(8) 0.2758(6) 0.070(3) Uani 1 1 d . . . C3 C 0.2280(11) 0.4995(11) 0.3393(6) 0.048(3) Uani 1 1 d . . . O3 O 0.2933(9) 0.5760(8) 0.3601(6) 0.072(3) Uani 1 1 d . . . C4 C -0.0033(11) 0.2457(10) 0.2423(7) 0.048(3) Uani 1 1 d . . . O4 O -0.0697(10) 0.1735(9) 0.2107(6) 0.077(3) Uani 1 1 d . . . C5 C 0.2593(12) 0.1336(11) 0.5382(8) 0.059(3) Uani 1 1 d . . . O5 O 0.3174(11) 0.0727(9) 0.5851(7) 0.090(3) Uani 1 1 d . . . C6 C 0.0350(13) 0.2735(12) 0.5369(8) 0.062(3) Uani 1 1 d . . . O6 O -0.0381(10) 0.2982(12) 0.5811(6) 0.097(4) Uani 1 1 d . . . C7 C 0.2795(12) 0.3660(11) 0.5116(6) 0.050(3) Uani 1 1 d . . . O7 O 0.3439(11) 0.4379(9) 0.5396(6) 0.090(4) Uani 1 1 d . . . C8 C 0.0485(12) 0.1114(12) 0.4141(7) 0.058(3) Uani 1 1 d . . . O8 O -0.0152(10) 0.0324(9) 0.3894(7) 0.091(3) Uani 1 1 d . . . C11 C 0.4401(9) 0.2841(8) 0.3632(6) 0.037(2) Uani 1 1 d . . . H11 H 0.4357 0.3584 0.3918 0.044 Uiso 1 1 calc R . . C12 C 0.4920(11) 0.3042(10) 0.2820(7) 0.048(3) Uani 1 1 d . . . H12A H 0.4368 0.3595 0.2484 0.058 Uiso 1 1 calc R . . H12B H 0.4896 0.2321 0.2512 0.058 Uiso 1 1 calc R . . C13 C 0.6323(12) 0.3502(13) 0.2975(8) 0.064(4) Uani 1 1 d . . . H13A H 0.6337 0.4259 0.3234 0.077 Uiso 1 1 calc R . . H13B H 0.6646 0.3584 0.2448 0.077 Uiso 1 1 calc R . . C14 C 0.7214(11) 0.2669(12) 0.3545(8) 0.064(4) Uani 1 1 d . . . H14A H 0.7265 0.1933 0.3264 0.076 Uiso 1 1 calc R . . H14B H 0.8084 0.2991 0.3660 0.076 Uiso 1 1 calc R . . C15 C 0.6687(11) 0.2480(10) 0.4360(8) 0.058(3) Uani 1 1 d . . . H15A H 0.6708 0.3205 0.4663 0.069 Uiso 1 1 calc R . . H15B H 0.7236 0.1930 0.4701 0.069 Uiso 1 1 calc R . . C16 C 0.5278(10) 0.2018(11) 0.4198(8) 0.054(3) Uani 1 1 d . . . H16A H 0.5267 0.1261 0.3938 0.065 Uiso 1 1 calc R . . H16B H 0.4949 0.1935 0.4723 0.065 Uiso 1 1 calc R . . H1 H 0.065(12) 0.347(9) 0.395(4) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0390(2) 0.0363(2) 0.0312(2) 0.00174(17) 0.00120(16) 0.00009(17) Re2 0.0432(2) 0.0402(3) 0.0327(2) 0.00366(18) 0.00541(17) 0.00116(19) S1 0.0385(13) 0.0363(12) 0.0379(14) -0.0056(11) 0.0061(11) -0.0004(11) C1 0.044(6) 0.049(6) 0.049(7) 0.006(6) -0.006(5) -0.001(5) O1 0.129(9) 0.085(7) 0.039(5) 0.014(5) 0.024(6) 0.000(6) C2 0.041(6) 0.043(6) 0.055(7) 0.011(5) -0.008(5) -0.010(5) O2 0.040(4) 0.063(5) 0.101(8) 0.019(5) -0.006(5) 0.006(4) C3 0.055(7) 0.054(7) 0.032(6) 0.004(5) 0.003(5) 0.001(6) O3 0.080(7) 0.066(6) 0.066(6) 0.005(5) -0.003(5) -0.014(5) C4 0.051(6) 0.056(7) 0.035(6) 0.005(5) -0.002(5) -0.008(6) O4 0.078(6) 0.077(7) 0.070(7) -0.019(5) -0.008(5) -0.024(6) C5 0.055(7) 0.062(8) 0.058(8) -0.004(7) 0.008(6) -0.005(7) O5 0.097(8) 0.084(7) 0.083(8) 0.040(6) -0.008(6) 0.008(6) C6 0.071(8) 0.080(9) 0.037(7) 0.012(6) 0.014(6) 0.008(7) O6 0.077(7) 0.164(11) 0.055(6) -0.019(7) 0.031(5) 0.010(7) C7 0.059(7) 0.068(8) 0.022(5) 0.001(5) 0.003(5) 0.003(6) O7 0.137(10) 0.077(7) 0.048(6) -0.014(5) -0.014(6) -0.050(7) C8 0.062(8) 0.077(9) 0.035(6) 0.012(6) 0.011(6) -0.008(7) O8 0.089(7) 0.067(6) 0.113(9) -0.003(6) 0.003(6) -0.040(6) C11 0.040(5) 0.028(5) 0.041(6) -0.004(4) 0.000(4) 0.006(4) C12 0.048(6) 0.051(7) 0.047(7) 0.001(5) 0.013(5) 0.004(5) C13 0.057(7) 0.080(10) 0.059(8) 0.000(7) 0.021(7) -0.014(7) C14 0.037(6) 0.077(9) 0.080(10) 0.000(8) 0.016(6) -0.012(6) C15 0.044(6) 0.056(8) 0.068(8) 0.001(6) -0.009(6) -0.001(6) C16 0.040(6) 0.060(7) 0.061(8) -0.001(6) 0.002(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.945(12) . ? Re1 C1 1.951(12) . ? Re1 C4 1.973(12) . ? Re1 C3 1.994(13) . ? Re1 S1 2.471(3) . ? Re1 Re2 3.0934(10) . ? Re2 C6 1.942(13) . ? Re2 C5 1.944(14) . ? Re2 C8 1.970(14) . ? Re2 C7 2.006(13) . ? Re2 S1 2.468(3) . ? S1 C11 1.817(10) . ? C1 O1 1.123(13) . ? C2 O2 1.144(13) . ? C3 O3 1.134(14) . ? C4 O4 1.153(13) . ? C5 O5 1.141(15) . ? C6 O6 1.157(14) . ? C7 O7 1.120(13) . ? C8 O8 1.163(15) . ? C11 C12 1.516(14) . ? C11 C16 1.526(15) . ? C12 C13 1.538(15) . ? C13 C14 1.544(18) . ? C14 C15 1.523(17) . ? C15 C16 1.545(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C1 94.8(5) . . ? C2 Re1 C4 88.0(5) . . ? C1 Re1 C4 87.6(5) . . ? C2 Re1 C3 91.2(5) . . ? C1 Re1 C3 89.9(4) . . ? C4 Re1 C3 177.3(4) . . ? C2 Re1 S1 165.2(3) . . ? C1 Re1 S1 99.5(3) . . ? C4 Re1 S1 88.9(3) . . ? C3 Re1 S1 92.5(3) . . ? C2 Re1 Re2 114.4(3) . . ? C1 Re1 Re2 150.7(3) . . ? C4 Re1 Re2 91.3(3) . . ? C3 Re1 Re2 91.4(3) . . ? S1 Re1 Re2 51.18(6) . . ? C6 Re2 C5 93.7(5) . . ? C6 Re2 C8 89.6(5) . . ? C5 Re2 C8 89.6(5) . . ? C6 Re2 C7 92.2(5) . . ? C5 Re2 C7 87.6(5) . . ? C8 Re2 C7 176.8(5) . . ? C6 Re2 S1 166.4(4) . . ? C5 Re2 S1 99.5(4) . . ? C8 Re2 S1 87.5(3) . . ? C7 Re2 S1 91.4(3) . . ? C6 Re2 Re1 115.5(4) . . ? C5 Re2 Re1 150.7(4) . . ? C8 Re2 Re1 90.8(3) . . ? C7 Re2 Re1 90.8(3) . . ? S1 Re2 Re1 51.26(6) . . ? C11 S1 Re2 112.1(3) . . ? C11 S1 Re1 112.0(3) . . ? Re2 S1 Re1 77.56(7) . . ? O1 C1 Re1 179.7(12) . . ? O2 C2 Re1 176.2(11) . . ? O3 C3 Re1 175.3(10) . . ? O4 C4 Re1 178.4(10) . . ? O5 C5 Re2 177.9(12) . . ? O6 C6 Re2 176.9(13) . . ? O7 C7 Re2 178.1(12) . . ? O8 C8 Re2 176.9(11) . . ? C12 C11 C16 111.2(9) . . ? C12 C11 S1 109.6(7) . . ? C16 C11 S1 109.0(7) . . ? C11 C12 C13 111.3(10) . . ? C12 C13 C14 110.6(10) . . ? C15 C14 C13 110.4(10) . . ? C14 C15 C16 110.9(10) . . ? C11 C16 C15 110.7(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.828 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.247 #=END data_2g _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_formula_sum 'C18 H8 O8 Re2 S' _chemical_formula_weight 756.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.047(3) _cell_length_b 16.792(4) _cell_length_c 16.853(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.23(2) _cell_angle_gamma 90.00 _cell_volume 1993.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.521 _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 12.279 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.625 _exptl_absorpt_correction_T_max 0.991 _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_decay_% 'less than 1' _diffrn_reflns_number 4746 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4599 _reflns_number_observed 3432 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4598 _refine_ls_number_parameters 263 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_obs 0.0452 _refine_ls_wR_factor_all 0.1274 _refine_ls_wR_factor_obs 0.1129 _refine_ls_goodness_of_fit_all 0.998 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 0.998 _refine_ls_restrained_S_obs 1.031 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.15121(6) 0.13971(2) 0.40504(2) 0.0349(2) Uani 1 d . . Re2 Re 0.15530(6) 0.20982(2) 0.23551(2) 0.03118(15) Uani 1 d . . S1 S 0.4279(4) 0.18235(14) 0.32727(14) 0.0341(5) Uani 1 d . . C1 C 0.1982(19) 0.0294(7) 0.3654(6) 0.050(3) Uani 1 d . . O1 O 0.2221(15) -0.0337(5) 0.3450(5) 0.065(3) Uani 1 d . . C2 C 0.2822(19) 0.1102(7) 0.5044(7) 0.049(3) Uani 1 d . . O2 O 0.3493(16) 0.0956(6) 0.5639(6) 0.074(3) Uani 1 d . . C3 C -0.0918(18) 0.1050(7) 0.4439(7) 0.049(3) Uani 1 d . . O3 O -0.2359(13) 0.0844(5) 0.4642(5) 0.065(3) Uani 1 d . . C4 C 0.1054(17) 0.2498(7) 0.4488(6) 0.044(3) Uani 1 d . . O4 O 0.0794(13) 0.3100(5) 0.4738(5) 0.053(2) Uani 1 d . . C5 C -0.0857(17) 0.2254(6) 0.1791(7) 0.042(2) Uani 1 d . . O5 O -0.2243(13) 0.2358(5) 0.1451(6) 0.059(2) Uani 1 d . . C6 C 0.1826(15) 0.1005(6) 0.1896(6) 0.036(2) Uani 1 d . . O6 O 0.2003(13) 0.0396(4) 0.1609(5) 0.051(2) Uani 1 d . . C7 C 0.1305(14) 0.3212(6) 0.2811(5) 0.031(2) Uani 1 d . . O7 O 0.1130(12) 0.3819(4) 0.3052(5) 0.049(2) Uani 1 d . . C8 C 0.2893(15) 0.2571(6) 0.1487(6) 0.038(2) Uani 1 d . . O8 O 0.3684(12) 0.2845(5) 0.0965(4) 0.051(2) Uani 1 d . . C11 C 0.5259(13) 0.2760(5) 0.3615(5) 0.030(2) Uani 1 d D . C12 C 0.5788(13) 0.3314(6) 0.3066(6) 0.036(2) Uani 1 d D . H12 H 0.5602(13) 0.3205(6) 0.2522(6) 0.043 Uiso 1 calc R . C13 C 0.6611(13) 0.4047(6) 0.3306(6) 0.035(2) Uani 1 d D . C14 C 0.7180(15) 0.4627(7) 0.2747(7) 0.043(3) Uani 1 d D . H14 H 0.7025(15) 0.4535(7) 0.2199(7) 0.052 Uiso 1 calc R . C15 C 0.7963(16) 0.5327(6) 0.3022(8) 0.047(3) Uani 1 d D . H15 H 0.8343(16) 0.5715(6) 0.2656(8) 0.057 Uiso 1 calc R . C16 C 0.8206(17) 0.5474(7) 0.3828(8) 0.051(3) Uani 1 d D . H16 H 0.8760(17) 0.5957(7) 0.3993(8) 0.061 Uiso 1 calc R . C17 C 0.7676(17) 0.4951(7) 0.4375(6) 0.049(3) Uani 1 d D . H17 H 0.7848(17) 0.5068(7) 0.4917(6) 0.059 Uiso 1 calc R . C18 C 0.6841(15) 0.4208(6) 0.4132(6) 0.042(2) Uani 1 d D . C19 C 0.6287(18) 0.3620(7) 0.4677(7) 0.051(3) Uani 1 d D . H19 H 0.6451(18) 0.3717(7) 0.5224(7) 0.061 Uiso 1 calc R . C20 C 0.5517(17) 0.2912(7) 0.4429(7) 0.046(3) Uani 1 d D . H20 H 0.5160(17) 0.2528(7) 0.4804(7) 0.056 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0461(3) 0.0287(2) 0.0302(2) 0.00085(15) 0.0104(2) -0.0018(2) Re2 0.0355(2) 0.0285(2) 0.0299(2) 0.00034(14) 0.0086(2) 0.0009(2) S1 0.0397(14) 0.0307(12) 0.0323(12) -0.0025(9) 0.0074(10) 0.0013(10) C1 0.074(9) 0.044(6) 0.032(5) 0.004(5) 0.019(6) 0.011(6) O1 0.110(8) 0.035(4) 0.052(5) -0.005(4) 0.015(5) 0.011(5) C2 0.075(9) 0.037(6) 0.036(6) 0.001(5) 0.014(6) 0.000(6) O2 0.112(9) 0.062(6) 0.046(5) 0.010(5) -0.015(5) 0.012(6) C3 0.058(8) 0.044(6) 0.047(6) 0.014(5) 0.017(6) -0.013(5) O3 0.066(6) 0.067(6) 0.062(5) 0.001(4) 0.022(5) -0.026(5) C4 0.054(7) 0.046(6) 0.032(5) 0.005(5) 0.018(5) -0.005(5) O4 0.071(6) 0.041(4) 0.047(5) -0.005(4) 0.019(4) 0.001(4) C5 0.051(7) 0.032(5) 0.043(6) -0.001(4) 0.009(5) 0.003(5) O5 0.048(5) 0.052(5) 0.077(6) -0.004(4) -0.006(5) 0.011(4) C6 0.039(6) 0.040(5) 0.029(5) 0.003(4) 0.008(4) 0.008(4) O6 0.070(6) 0.035(4) 0.050(5) -0.007(3) 0.009(4) 0.000(4) C7 0.034(5) 0.036(5) 0.023(4) -0.004(4) 0.004(4) 0.005(4) O7 0.051(5) 0.036(4) 0.059(5) -0.006(4) 0.011(4) 0.004(4) C8 0.038(6) 0.037(5) 0.038(5) -0.002(4) 0.005(4) 0.000(4) O8 0.058(5) 0.059(5) 0.039(4) 0.008(4) 0.020(4) 0.001(4) C11 0.030(5) 0.028(4) 0.031(5) -0.001(4) 0.005(4) 0.000(4) C12 0.035(5) 0.042(5) 0.030(5) 0.001(4) 0.001(4) 0.003(4) C13 0.033(5) 0.033(5) 0.039(5) 0.004(4) 0.014(4) 0.007(4) C14 0.037(6) 0.050(6) 0.043(6) 0.004(5) 0.008(5) 0.005(5) C15 0.039(6) 0.036(6) 0.067(8) 0.000(5) 0.008(5) -0.007(5) C16 0.043(6) 0.036(6) 0.075(9) -0.005(6) 0.003(6) -0.002(5) C17 0.057(7) 0.054(7) 0.035(6) -0.016(5) -0.001(5) -0.006(6) C18 0.039(6) 0.038(6) 0.049(6) -0.004(5) 0.010(5) 0.002(5) C19 0.061(8) 0.057(7) 0.035(6) -0.002(5) 0.007(5) -0.009(6) C20 0.052(7) 0.052(7) 0.035(6) 0.006(5) 0.010(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.936(11) . ? Re1 C2 1.959(13) . ? Re1 C1 1.999(11) . ? Re1 C4 2.018(12) . ? Re1 S1 2.478(3) . ? Re1 Re2 3.0909(8) . ? Re2 C8 1.929(10) . ? Re2 C5 1.946(13) . ? Re2 C6 2.002(10) . ? Re2 C7 2.031(10) . ? Re2 S1 2.483(3) . ? S1 C11 1.808(9) . ? C1 O1 1.128(13) . ? C2 O2 1.127(14) . ? C3 O3 1.133(13) . ? C4 O4 1.113(13) . ? C5 O5 1.135(14) . ? C6 O6 1.139(12) . ? C7 O7 1.105(12) . ? C8 O8 1.148(12) . ? C11 C12 1.369(13) . ? C11 C20 1.403(14) . ? C12 C13 1.417(14) . ? C13 C14 1.419(14) . ? C13 C18 1.424(15) . ? C14 C15 1.375(15) . ? C15 C16 1.39(2) . ? C16 C17 1.33(2) . ? C17 C18 1.436(15) . ? C18 C19 1.409(15) . ? C19 C20 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re1 C2 92.2(5) . . ? C3 Re1 C1 89.3(5) . . ? C2 Re1 C1 88.4(5) . . ? C3 Re1 C4 90.2(5) . . ? C2 Re1 C4 89.7(5) . . ? C1 Re1 C4 178.0(4) . . ? C3 Re1 S1 167.8(4) . . ? C2 Re1 S1 99.4(4) . . ? C1 Re1 S1 87.3(3) . . ? C4 Re1 S1 93.6(3) . . ? C3 Re1 Re2 116.9(4) . . ? C2 Re1 Re2 150.8(4) . . ? C1 Re1 Re2 92.3(3) . . ? C4 Re1 Re2 89.7(3) . . ? S1 Re1 Re2 51.54(6) . . ? C8 Re2 C5 90.6(5) . . ? C8 Re2 C6 91.8(4) . . ? C5 Re2 C6 91.4(4) . . ? C8 Re2 C7 87.5(4) . . ? C5 Re2 C7 88.8(4) . . ? C6 Re2 C7 179.2(4) . . ? C8 Re2 S1 99.4(3) . . ? C5 Re2 S1 169.9(3) . . ? C6 Re2 S1 89.5(3) . . ? C7 Re2 S1 90.4(3) . . ? C8 Re2 Re1 150.7(3) . . ? C5 Re2 Re1 118.5(3) . . ? C6 Re2 Re1 90.6(3) . . ? C7 Re2 Re1 89.9(3) . . ? S1 Re2 Re1 51.39(6) . . ? C11 S1 Re1 112.5(3) . . ? C11 S1 Re2 108.8(3) . . ? Re1 S1 Re2 77.07(8) . . ? O1 C1 Re1 178.0(10) . . ? O2 C2 Re1 175.9(11) . . ? O3 C3 Re1 177.9(11) . . ? O4 C4 Re1 179.1(9) . . ? O5 C5 Re2 178.3(10) . . ? O6 C6 Re2 177.4(8) . . ? O7 C7 Re2 178.4(9) . . ? O8 C8 Re2 179.2(10) . . ? C12 C11 C20 120.4(9) . . ? C12 C11 S1 118.8(7) . . ? C20 C11 S1 120.7(7) . . ? C11 C12 C13 120.8(9) . . ? C12 C13 C14 121.8(10) . . ? C12 C13 C18 118.7(9) . . ? C14 C13 C18 119.4(10) . . ? C15 C14 C13 118.7(11) . . ? C14 C15 C16 121.5(11) . . ? C17 C16 C15 122.0(11) . . ? C16 C17 C18 119.7(10) . . ? C19 C18 C13 118.6(10) . . ? C19 C18 C17 122.7(10) . . ? C13 C18 C17 118.7(10) . . ? C20 C19 C18 121.5(11) . . ? C19 C20 C11 119.9(10) . . ? _refine_diff_density_max 0.981 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.273 #=END data_5a _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H22 Au O8 P Re2 S' _chemical_formula_weight 1214.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5182(13) _cell_length_b 12.435(3) _cell_length_c 14.8394(17) _cell_angle_alpha 85.642(14) _cell_angle_beta 68.170(9) _cell_angle_gamma 64.389(14) _cell_volume 1770.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 9.77 _cell_measurement_theta_max 20.01 _exptl_crystal_description 'block ' _exptl_crystal_colour 'yellow ' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 2.279 _exptl_crystal_density_meas not_measured _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 11.110 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.987 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Bruker AXS P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 'less than 1' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 9248 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8053 _reflns_number_gt 6713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1028P)^2^+0.7841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8053 _refine_ls_number_parameters 443 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.88927(4) 0.45774(3) -0.68743(2) 0.03869(13) Uani 1 1 d . . . Re1 Re 1.02600(4) 0.31878(3) -0.86646(2) 0.03670(13) Uani 1 1 d . . . Re2 Re 0.82634(4) 0.26177(3) -0.67989(3) 0.04022(13) Uani 1 1 d . . . S1 S 0.9583(2) 0.1525(2) -0.84443(17) 0.0418(5) Uani 1 1 d . . . P1 P 0.7976(3) 0.6438(2) -0.60250(17) 0.0401(5) Uani 1 1 d . . . C1 C 1.1894(10) 0.1997(10) -0.8387(7) 0.051(2) Uani 1 1 d . . . O1 O 1.2838(9) 0.1303(9) -0.8246(7) 0.081(3) Uani 1 1 d . . . C2 C 0.8591(11) 0.4499(8) -0.8809(7) 0.046(2) Uani 1 1 d . . . O2 O 0.7640(8) 0.5307(7) -0.8874(6) 0.062(2) Uani 1 1 d . . . C3 C 1.1194(13) 0.2737(9) -1.0037(8) 0.058(3) Uani 1 1 d . . . O3 O 1.1790(10) 0.2472(9) -1.0865(5) 0.075(2) Uani 1 1 d . . . C4 C 1.0993(10) 0.4359(10) -0.8757(7) 0.049(2) Uani 1 1 d . . . O4 O 1.1478(10) 0.5009(8) -0.8870(6) 0.071(2) Uani 1 1 d . . . C5 C 0.9882(12) 0.1648(10) -0.6466(7) 0.053(2) Uani 1 1 d . . . O5 O 1.0801(11) 0.1060(9) -0.6244(7) 0.083(3) Uani 1 1 d . . . C6 C 0.6643(10) 0.3700(9) -0.7180(8) 0.051(2) Uani 1 1 d . . . O6 O 0.5752(8) 0.4309(8) -0.7370(7) 0.066(2) Uani 1 1 d . . . C7 C 0.7474(11) 0.1501(9) -0.6309(8) 0.052(2) Uani 1 1 d . . . O7 O 0.7013(10) 0.0847(8) -0.6032(7) 0.079(3) Uani 1 1 d . . . C8 C 0.7263(12) 0.3597(10) -0.5541(7) 0.053(2) Uani 1 1 d . . . O8 O 0.6631(11) 0.4094(9) -0.4780(6) 0.081(3) Uani 1 1 d . . . C11 C 0.7441(9) 0.6460(7) -0.4708(6) 0.044(2) Uani 1 1 d D . . C12 C 0.6312(10) 0.7429(9) -0.4081(7) 0.063(3) Uani 1 1 d D . . H12 H 0.5817 0.8101 -0.4334 0.076 Uiso 1 1 calc R . . C13 C 0.5920(12) 0.7400(10) -0.3085(7) 0.070(3) Uani 1 1 d D . . H13 H 0.5137 0.8042 -0.2674 0.083 Uiso 1 1 calc R . . C14 C 0.6653(12) 0.6453(10) -0.2691(8) 0.067(3) Uani 1 1 d D . . H14 H 0.6426 0.6472 -0.2020 0.080 Uiso 1 1 calc R . . C15 C 0.7725(11) 0.5477(10) -0.3297(7) 0.063(3) Uani 1 1 d D . . H15 H 0.8191 0.4803 -0.3031 0.075 Uiso 1 1 calc R . . C16 C 0.8140(11) 0.5466(9) -0.4305(7) 0.056(3) Uani 1 1 d D . . H16 H 0.8884 0.4794 -0.4707 0.067 Uiso 1 1 calc R . . C21 C 0.6416(9) 0.7425(7) -0.6266(6) 0.044(2) Uani 1 1 d D . . C22 C 0.5654(10) 0.6893(8) -0.6425(7) 0.054(2) Uani 1 1 d D . . H22 H 0.5905 0.6080 -0.6369 0.065 Uiso 1 1 calc R . . C23 C 0.4512(11) 0.7597(10) -0.6670(9) 0.073(3) Uani 1 1 d D . . H23 H 0.4000 0.7248 -0.6778 0.087 Uiso 1 1 calc R . . C24 C 0.4139(13) 0.8772(10) -0.6753(10) 0.077(4) Uani 1 1 d D . . H24 H 0.3367 0.9233 -0.6908 0.093 Uiso 1 1 calc R . . C25 C 0.4888(15) 0.9280(11) -0.6609(13) 0.091(5) Uani 1 1 d D . . H25 H 0.4630 1.0091 -0.6682 0.110 Uiso 1 1 calc R . . C26 C 0.6024(13) 0.8638(8) -0.6358(10) 0.072(4) Uani 1 1 d D . . H26 H 0.6517 0.9011 -0.6253 0.087 Uiso 1 1 calc R . . C31 C 0.9045(9) 0.7247(8) -0.6392(6) 0.043(2) Uani 1 1 d D . . C32 C 0.9495(10) 0.7447(8) -0.7374(6) 0.051(2) Uani 1 1 d D . . H32 H 0.9235 0.7187 -0.7806 0.062 Uiso 1 1 calc R . . C33 C 1.0332(12) 0.8036(10) -0.7696(8) 0.068(3) Uani 1 1 d D . . H33 H 1.0631 0.8169 -0.8350 0.081 Uiso 1 1 calc R . . C34 C 1.0732(13) 0.8427(11) -0.7080(8) 0.069(3) Uani 1 1 d D . . H34 H 1.1304 0.8814 -0.7311 0.082 Uiso 1 1 calc R . . C35 C 1.0278(17) 0.8241(14) -0.6117(8) 0.088(5) Uani 1 1 d D . . H35 H 1.0544 0.8509 -0.5693 0.106 Uiso 1 1 calc R . . C36 C 0.9431(12) 0.7664(10) -0.5760(7) 0.059(3) Uani 1 1 d D . . H36 H 0.9121 0.7556 -0.5101 0.071 Uiso 1 1 calc R . . C41 C 0.8405(9) 0.1577(8) -0.8964(6) 0.0423(19) Uani 1 1 d D . . C42 C 0.7878(9) 0.2453(8) -0.9509(6) 0.046(2) Uani 1 1 d D . . H42 H 0.8161 0.3064 -0.9632 0.055 Uiso 1 1 calc R . . C43 C 0.6908(9) 0.2463(9) -0.9898(6) 0.048(2) Uani 1 1 d D . . C44 C 0.6356(12) 0.3361(11) -1.0458(9) 0.065(3) Uani 1 1 d D . . H44 H 0.6627 0.3979 -1.0584 0.078 Uiso 1 1 calc R . . C45 C 0.5427(16) 0.3348(15) -1.0822(11) 0.086(4) Uani 1 1 d D . . H45 H 0.5058 0.3960 -1.1178 0.103 Uiso 1 1 calc R . . C46 C 0.5050(14) 0.2428(15) -1.0656(10) 0.086(4) Uani 1 1 d D . . H46 H 0.4420 0.2411 -1.0899 0.103 Uiso 1 1 calc R . . C47 C 0.5592(13) 0.1538(14) -1.0137(10) 0.076(4) Uani 1 1 d D . . H47 H 0.5335 0.0913 -1.0049 0.091 Uiso 1 1 calc R . . C48 C 0.6518(11) 0.1512(10) -0.9728(8) 0.057(3) Uani 1 1 d D . . C49 C 0.7072(14) 0.0628(11) -0.9166(9) 0.065(3) Uani 1 1 d D . . H49 H 0.6808 0.0006 -0.9039 0.079 Uiso 1 1 calc R . . C50 C 0.7993(12) 0.0652(9) -0.8797(8) 0.057(3) Uani 1 1 d D . . H50 H 0.8345 0.0046 -0.8431 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0385(2) 0.0375(2) 0.03869(19) -0.00155(13) -0.01276(15) -0.01612(15) Re1 0.0355(2) 0.0429(2) 0.03292(19) 0.00091(13) -0.01141(14) -0.01886(16) Re2 0.0420(2) 0.0409(2) 0.0386(2) 0.00286(14) -0.01131(16) -0.02182(17) S1 0.0419(12) 0.0395(11) 0.0442(11) -0.0001(9) -0.0179(10) -0.0158(10) P1 0.0406(13) 0.0390(11) 0.0391(11) -0.0025(9) -0.0124(10) -0.0171(10) C1 0.037(5) 0.067(6) 0.048(5) 0.003(5) -0.019(4) -0.020(5) O1 0.058(5) 0.090(7) 0.084(6) 0.020(5) -0.034(5) -0.019(5) C2 0.056(6) 0.045(5) 0.051(5) 0.014(4) -0.027(5) -0.031(5) O2 0.063(5) 0.052(4) 0.076(5) 0.021(4) -0.036(4) -0.022(4) C3 0.082(8) 0.051(6) 0.053(6) -0.003(5) -0.031(6) -0.034(6) O3 0.088(7) 0.099(6) 0.035(4) -0.007(4) -0.007(4) -0.049(6) C4 0.043(5) 0.069(6) 0.039(5) 0.002(4) -0.011(4) -0.030(5) O4 0.080(6) 0.075(5) 0.073(5) 0.004(4) -0.013(5) -0.059(5) C5 0.059(6) 0.061(6) 0.040(5) 0.000(4) -0.021(5) -0.025(5) O5 0.093(7) 0.098(7) 0.065(5) 0.011(5) -0.047(5) -0.033(6) C6 0.037(5) 0.055(6) 0.062(6) 0.001(5) -0.015(5) -0.023(5) O6 0.043(4) 0.071(5) 0.084(6) 0.022(4) -0.028(4) -0.023(4) C7 0.049(6) 0.043(5) 0.058(6) 0.001(4) -0.012(5) -0.021(5) O7 0.080(6) 0.060(5) 0.095(7) 0.013(5) -0.014(5) -0.047(5) C8 0.055(6) 0.066(6) 0.038(5) -0.002(4) -0.007(5) -0.034(5) O8 0.089(7) 0.082(6) 0.058(5) -0.015(4) 0.006(5) -0.051(6) C11 0.043(5) 0.043(5) 0.039(4) -0.003(4) -0.012(4) -0.015(4) C12 0.053(7) 0.054(6) 0.057(6) -0.012(5) -0.013(5) -0.005(5) C13 0.063(8) 0.070(7) 0.051(6) -0.017(5) -0.001(6) -0.022(6) C14 0.064(8) 0.087(9) 0.048(6) -0.003(6) -0.021(6) -0.030(7) C15 0.053(7) 0.078(8) 0.058(6) 0.017(6) -0.024(5) -0.028(6) C16 0.049(6) 0.066(7) 0.049(5) 0.001(5) -0.018(5) -0.022(5) C21 0.048(5) 0.039(4) 0.047(5) 0.005(4) -0.019(4) -0.020(4) C22 0.053(6) 0.050(5) 0.074(7) 0.015(5) -0.033(6) -0.027(5) C23 0.050(7) 0.074(8) 0.105(10) 0.013(7) -0.040(7) -0.028(6) C24 0.067(8) 0.066(8) 0.096(10) 0.024(7) -0.049(8) -0.014(7) C25 0.096(11) 0.060(8) 0.135(14) 0.036(8) -0.062(11) -0.037(8) C26 0.071(8) 0.040(5) 0.112(11) 0.011(6) -0.043(8) -0.023(6) C31 0.040(5) 0.050(5) 0.037(4) -0.002(4) -0.007(4) -0.022(4) C32 0.054(6) 0.066(6) 0.043(5) 0.011(4) -0.021(5) -0.033(5) C33 0.075(8) 0.070(7) 0.048(6) 0.012(5) -0.013(6) -0.032(7) C34 0.064(8) 0.069(7) 0.078(8) 0.011(6) -0.019(7) -0.041(7) C35 0.127(13) 0.126(12) 0.062(7) 0.010(8) -0.032(8) -0.103(11) C36 0.073(8) 0.083(8) 0.038(5) 0.005(5) -0.018(5) -0.053(7) C41 0.033(4) 0.053(5) 0.039(4) -0.006(4) -0.008(4) -0.020(4) C42 0.053(6) 0.052(5) 0.047(5) 0.013(4) -0.021(4) -0.035(5) C43 0.042(5) 0.056(6) 0.045(5) 0.000(4) -0.012(4) -0.024(5) C44 0.061(7) 0.074(8) 0.079(8) 0.015(6) -0.039(7) -0.036(6) C45 0.077(9) 0.107(11) 0.089(10) 0.006(8) -0.038(8) -0.045(9) C46 0.058(8) 0.130(13) 0.084(9) -0.005(9) -0.037(7) -0.044(9) C47 0.061(8) 0.099(10) 0.078(8) -0.016(7) -0.016(7) -0.049(8) C48 0.038(5) 0.065(6) 0.059(6) -0.020(5) -0.009(5) -0.019(5) C49 0.078(8) 0.060(6) 0.080(8) 0.005(6) -0.033(7) -0.046(6) C50 0.066(7) 0.041(5) 0.062(6) -0.002(5) -0.023(6) -0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.324(2) . ? Au1 Re1 2.7853(8) . ? Au1 Re2 2.8110(7) . ? Re1 C3 1.909(11) . ? Re1 C4 1.949(10) . ? Re1 C2 1.986(10) . ? Re1 C1 1.995(10) . ? Re1 S1 2.469(2) . ? Re1 Re2 3.1356(7) . ? Re2 C7 1.931(10) . ? Re2 C5 1.956(11) . ? Re2 C8 1.957(10) . ? Re2 C6 2.028(10) . ? Re2 S1 2.465(2) . ? S1 C41 1.769(9) . ? P1 C11 1.816(9) . ? P1 C31 1.820(9) . ? P1 C21 1.834(9) . ? C1 O1 1.140(12) . ? C2 O2 1.154(11) . ? C3 O3 1.151(13) . ? C4 O4 1.138(12) . ? C5 O5 1.147(13) . ? C6 O6 1.102(12) . ? C7 O7 1.128(12) . ? C8 O8 1.137(13) . ? C11 C16 1.386(10) . ? C11 C12 1.387(10) . ? C12 C13 1.378(11) . ? C13 C14 1.358(12) . ? C14 C15 1.361(11) . ? C15 C16 1.389(11) . ? C21 C26 1.386(10) . ? C21 C22 1.395(10) . ? C22 C23 1.393(11) . ? C23 C24 1.343(11) . ? C24 C25 1.348(12) . ? C25 C26 1.380(12) . ? C31 C36 1.389(10) . ? C31 C32 1.396(10) . ? C32 C33 1.381(11) . ? C33 C34 1.363(12) . ? C34 C35 1.366(12) . ? C35 C36 1.383(11) . ? C41 C42 1.367(13) . ? C41 C50 1.397(14) . ? C42 C43 1.432(13) . ? C43 C44 1.406(15) . ? C43 C48 1.411(15) . ? C44 C45 1.373(17) . ? C45 C46 1.37(2) . ? C46 C47 1.36(2) . ? C47 C48 1.398(16) . ? C48 C49 1.400(17) . ? C49 C50 1.374(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Re1 148.14(6) . . ? P1 Au1 Re2 139.18(6) . . ? Re1 Au1 Re2 68.151(19) . . ? C3 Re1 C4 91.1(4) . . ? C3 Re1 C2 93.0(5) . . ? C4 Re1 C2 87.7(4) . . ? C3 Re1 C1 92.7(5) . . ? C4 Re1 C1 88.3(4) . . ? C2 Re1 C1 173.1(4) . . ? C3 Re1 S1 91.1(3) . . ? C4 Re1 S1 171.7(3) . . ? C2 Re1 S1 100.2(3) . . ? C1 Re1 S1 83.6(3) . . ? C3 Re1 Au1 160.6(3) . . ? C4 Re1 Au1 72.3(3) . . ? C2 Re1 Au1 76.8(3) . . ? C1 Re1 Au1 96.6(3) . . ? S1 Re1 Au1 106.81(6) . . ? C3 Re1 Re2 140.9(3) . . ? C4 Re1 Re2 128.0(3) . . ? C2 Re1 Re2 88.2(3) . . ? C1 Re1 Re2 89.9(3) . . ? S1 Re1 Re2 50.49(6) . . ? Au1 Re1 Re2 56.314(17) . . ? C7 Re2 C5 91.3(5) . . ? C7 Re2 C8 92.2(4) . . ? C5 Re2 C8 92.3(4) . . ? C7 Re2 C6 92.5(4) . . ? C5 Re2 C6 176.1(4) . . ? C8 Re2 C6 87.6(5) . . ? C7 Re2 S1 92.7(3) . . ? C5 Re2 S1 88.4(3) . . ? C8 Re2 S1 175.0(3) . . ? C6 Re2 S1 91.4(3) . . ? C7 Re2 Au1 161.1(3) . . ? C5 Re2 Au1 88.9(3) . . ? C8 Re2 Au1 68.9(3) . . ? C6 Re2 Au1 87.4(3) . . ? S1 Re2 Au1 106.13(6) . . ? C7 Re2 Re1 143.3(3) . . ? C5 Re2 Re1 87.9(3) . . ? C8 Re2 Re1 124.5(3) . . ? C6 Re2 Re1 88.9(3) . . ? S1 Re2 Re1 50.59(6) . . ? Au1 Re2 Re1 55.535(18) . . ? C41 S1 Re2 109.2(3) . . ? C41 S1 Re1 117.9(3) . . ? Re2 S1 Re1 78.91(7) . . ? C11 P1 C31 105.4(4) . . ? C11 P1 C21 106.5(4) . . ? C31 P1 C21 103.7(4) . . ? C11 P1 Au1 115.8(3) . . ? C31 P1 Au1 116.8(3) . . ? C21 P1 Au1 107.5(3) . . ? O1 C1 Re1 178.6(10) . . ? O2 C2 Re1 176.1(8) . . ? O3 C3 Re1 177.9(11) . . ? O4 C4 Re1 175.5(9) . . ? O5 C5 Re2 177.3(11) . . ? O6 C6 Re2 178.3(10) . . ? O7 C7 Re2 179.3(10) . . ? O8 C8 Re2 173.8(10) . . ? C16 C11 C12 118.2(8) . . ? C16 C11 P1 119.6(6) . . ? C12 C11 P1 122.1(7) . . ? C13 C12 C11 120.4(9) . . ? C14 C13 C12 121.3(9) . . ? C13 C14 C15 118.7(10) . . ? C14 C15 C16 121.4(9) . . ? C11 C16 C15 119.7(9) . . ? C26 C21 C22 119.3(9) . . ? C26 C21 P1 123.4(7) . . ? C22 C21 P1 117.2(6) . . ? C21 C22 C23 119.0(9) . . ? C24 C23 C22 121.1(10) . . ? C23 C24 C25 119.7(10) . . ? C24 C25 C26 122.2(10) . . ? C25 C26 C21 118.6(10) . . ? C36 C31 C32 119.0(8) . . ? C36 C31 P1 124.1(6) . . ? C32 C31 P1 116.8(6) . . ? C33 C32 C31 119.3(8) . . ? C34 C33 C32 121.7(9) . . ? C33 C34 C35 118.9(10) . . ? C34 C35 C36 121.3(10) . . ? C35 C36 C31 119.7(9) . . ? C42 C41 C50 118.4(9) . . ? C42 C41 S1 124.7(7) . . ? C50 C41 S1 116.9(8) . . ? C41 C42 C43 122.4(9) . . ? C44 C43 C48 119.0(9) . . ? C44 C43 C42 122.8(9) . . ? C48 C43 C42 118.2(9) . . ? C45 C44 C43 121.6(13) . . ? C46 C45 C44 119.3(14) . . ? C47 C46 C45 120.1(12) . . ? C46 C47 C48 123.5(13) . . ? C47 C48 C49 125.2(12) . . ? C47 C48 C43 116.5(12) . . ? C49 C48 C43 118.3(9) . . ? C50 C49 C48 122.0(10) . . ? C49 C50 C41 120.8(10) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.746 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.329 #=END data_5b _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H22 Ag O8 P Re2 S' _chemical_formula_weight 1125.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.380(2) _cell_length_b 12.439(2) _cell_length_c 14.722(4) _cell_angle_alpha 76.80(2) _cell_angle_beta 67.37(2) _cell_angle_gamma 64.24(2) _cell_volume 1727.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 14.298 _cell_measurement_theta_max 38.355 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 2.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 7.709 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.701 _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 'less than 1' _diffrn_reflns_number 9098 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7909 _reflns_number_gt 6538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.1527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00394(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7909 _refine_ls_number_parameters 443 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.16238(2) 0.815231(17) 0.367823(13) 0.02123(6) Uani 1 1 d . . . Re2 Re 0.15423(2) 0.755092(17) 0.177262(14) 0.02386(6) Uani 1 1 d . . . Ag1 Ag 0.22152(4) 0.94747(3) 0.18495(3) 0.02535(9) Uani 1 1 d . . . S1 S 0.11850(13) 0.64839(11) 0.34317(9) 0.0247(3) Uani 1 1 d . . . P1 P 0.20734(14) 1.14336(11) 0.09803(9) 0.0242(3) Uani 1 1 d . . . O1 O 0.0855(5) 0.7536(4) 0.5926(3) 0.0453(10) Uani 1 1 d . . . C1 C 0.1149(5) 0.7762(5) 0.5084(4) 0.0288(11) Uani 1 1 d . . . O2 O 0.2589(4) 1.0017(4) 0.3910(3) 0.0414(10) Uani 1 1 d . . . C2 C 0.2240(6) 0.9342(5) 0.3776(4) 0.0302(12) Uani 1 1 d . . . O3 O -0.1196(4) 1.0287(3) 0.3805(3) 0.0389(9) Uani 1 1 d . . . C3 C -0.0190(5) 0.9483(5) 0.3762(4) 0.0271(11) Uani 1 1 d . . . C4 C 0.3555(6) 0.6937(5) 0.3411(4) 0.0290(11) Uani 1 1 d . . . O4 O 0.4650(4) 0.6254(4) 0.3268(3) 0.0475(11) Uani 1 1 d . . . C5 C 0.3531(6) 0.6545(5) 0.1451(4) 0.0319(12) Uani 1 1 d . . . O5 O 0.4676(4) 0.5954(4) 0.1249(3) 0.0490(11) Uani 1 1 d . . . C6 C -0.0447(6) 0.8645(5) 0.2131(4) 0.0317(12) Uani 1 1 d . . . O6 O -0.1571(4) 0.9278(4) 0.2301(3) 0.0447(10) Uani 1 1 d . . . O7 O 0.1091(5) 0.5799(4) 0.0895(3) 0.0525(12) Uani 1 1 d . . . C7 C 0.1268(6) 0.6455(5) 0.1214(4) 0.0341(12) Uani 1 1 d . . . O8 O 0.1929(5) 0.9063(4) -0.0226(3) 0.0538(13) Uani 1 1 d . . . C8 C 0.1831(6) 0.8515(5) 0.0523(4) 0.0361(13) Uani 1 1 d . . . C11 C 0.2739(5) 1.2271(4) 0.1374(3) 0.0268(11) Uani 1 1 d D . . C12 C 0.3796(5) 1.2654(5) 0.0744(4) 0.0343(13) Uani 1 1 d D . . H12 H 0.4165 1.2520 0.0070 0.041 Uiso 1 1 calc R . . C13 C 0.4290(6) 1.3231(5) 0.1122(4) 0.0415(14) Uani 1 1 d D . . H13 H 0.5002 1.3484 0.0703 0.050 Uiso 1 1 calc R . . C14 C 0.3746(6) 1.3438(5) 0.2109(4) 0.0386(13) Uani 1 1 d D . . H14 H 0.4092 1.3830 0.2357 0.046 Uiso 1 1 calc R . . C15 C 0.2702(6) 1.3077(5) 0.2734(4) 0.0390(13) Uani 1 1 d D . . H15 H 0.2322 1.3234 0.3404 0.047 Uiso 1 1 calc R . . C16 C 0.2220(6) 1.2485(5) 0.2369(4) 0.0334(12) Uani 1 1 d D . . H16 H 0.1526 1.2218 0.2800 0.040 Uiso 1 1 calc R . . C21 C 0.2810(5) 1.1482(4) -0.0362(3) 0.0247(10) Uani 1 1 d D . . C22 C 0.3909(5) 1.0484(5) -0.0797(4) 0.0320(12) Uani 1 1 d D . . H22 H 0.4260 0.9801 -0.0399 0.038 Uiso 1 1 calc R . . C23 C 0.4500(6) 1.0480(5) -0.1816(4) 0.0390(13) Uani 1 1 d D . . H23 H 0.5245 0.9797 -0.2105 0.047 Uiso 1 1 calc R . . C24 C 0.3990(6) 1.1483(5) -0.2404(4) 0.0380(13) Uani 1 1 d D . . H24 H 0.4402 1.1492 -0.3094 0.046 Uiso 1 1 calc R . . C25 C 0.2889(6) 1.2461(5) -0.1982(4) 0.0403(14) Uani 1 1 d D . . H25 H 0.2534 1.3133 -0.2387 0.048 Uiso 1 1 calc R . . C26 C 0.2283(6) 1.2482(5) -0.0966(4) 0.0345(12) Uani 1 1 d D . . H26 H 0.1524 1.3163 -0.0686 0.041 Uiso 1 1 calc R . . C31 C 0.0242(5) 1.2371(4) 0.1272(3) 0.0264(10) Uani 1 1 d D . . C32 C -0.0669(5) 1.1832(5) 0.1440(4) 0.0332(12) Uani 1 1 d D . . H32 H -0.0319 1.1009 0.1362 0.040 Uiso 1 1 calc R . . C33 C -0.2068(6) 1.2468(5) 0.1718(4) 0.0411(14) Uani 1 1 d D . . H33 H -0.2666 1.2081 0.1830 0.049 Uiso 1 1 calc R . . C34 C -0.2595(6) 1.3675(5) 0.1833(4) 0.0451(15) Uani 1 1 d D . . H34 H -0.3553 1.4117 0.2031 0.054 Uiso 1 1 calc R . . C35 C -0.1701(6) 1.4220(5) 0.1654(5) 0.0507(17) Uani 1 1 d D . . H35 H -0.2057 1.5045 0.1726 0.061 Uiso 1 1 calc R . . C36 C -0.0294(6) 1.3589(5) 0.1370(5) 0.0420(14) Uani 1 1 d D . . H36 H 0.0300 1.3984 0.1243 0.050 Uiso 1 1 calc R . . C41 C -0.0555(5) 0.6578(4) 0.3949(3) 0.0251(10) Uani 1 1 d D . . C42 C -0.1629(5) 0.7482(4) 0.4483(3) 0.0284(11) Uani 1 1 d D . . H42 H -0.1471 0.8117 0.4592 0.034 Uiso 1 1 calc R . . C43 C -0.2986(5) 0.7488(4) 0.4882(3) 0.0275(11) Uani 1 1 d D . . C44 C -0.4121(6) 0.8436(5) 0.5408(4) 0.0376(13) Uani 1 1 d D . . H44 H -0.3990 0.9096 0.5496 0.045 Uiso 1 1 calc R . . C45 C -0.5404(6) 0.8409(6) 0.5791(5) 0.0464(15) Uani 1 1 d D . . H45 H -0.6150 0.9048 0.6143 0.056 Uiso 1 1 calc R . . C46 C -0.5620(6) 0.7436(6) 0.5663(4) 0.0441(15) Uani 1 1 d D . . H46 H -0.6508 0.7420 0.5935 0.053 Uiso 1 1 calc R . . C47 C -0.4552(6) 0.6515(6) 0.5145(4) 0.0396(14) Uani 1 1 d D . . H47 H -0.4713 0.5869 0.5061 0.048 Uiso 1 1 calc R . . C48 C -0.3203(5) 0.6510(5) 0.4730(4) 0.0294(11) Uani 1 1 d D . . C49 C -0.2062(6) 0.5585(5) 0.4180(4) 0.0365(13) Uani 1 1 d D . . H49 H -0.2192 0.4933 0.4076 0.044 Uiso 1 1 calc R . . C50 C -0.0773(6) 0.5606(5) 0.3793(4) 0.0329(12) Uani 1 1 d D . . H50 H -0.0032 0.4978 0.3425 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01952(11) 0.02435(11) 0.01913(10) 0.00070(7) -0.00360(8) -0.01129(8) Re2 0.02655(12) 0.02423(11) 0.02232(11) -0.00036(8) -0.00607(8) -0.01342(9) Ag1 0.0293(2) 0.02353(18) 0.02301(18) 0.00343(14) -0.00657(16) -0.01420(16) S1 0.0229(6) 0.0227(6) 0.0258(6) 0.0014(5) -0.0045(5) -0.0108(5) P1 0.0240(7) 0.0225(6) 0.0239(6) 0.0033(5) -0.0052(5) -0.0118(5) O1 0.056(3) 0.058(3) 0.024(2) 0.0075(18) -0.008(2) -0.033(2) C1 0.030(3) 0.031(3) 0.027(3) 0.001(2) -0.005(2) -0.018(2) O2 0.049(3) 0.053(2) 0.036(2) -0.0034(19) -0.010(2) -0.036(2) C2 0.036(3) 0.039(3) 0.022(2) 0.004(2) -0.008(2) -0.024(3) O3 0.029(2) 0.034(2) 0.048(2) -0.0090(18) -0.0078(19) -0.0085(19) C3 0.028(3) 0.030(3) 0.024(3) -0.002(2) -0.006(2) -0.015(2) C4 0.026(3) 0.030(3) 0.029(3) -0.001(2) -0.009(2) -0.010(2) O4 0.030(2) 0.048(3) 0.055(3) -0.007(2) -0.016(2) -0.004(2) C5 0.035(3) 0.031(3) 0.028(3) 0.001(2) -0.006(2) -0.018(3) O5 0.029(2) 0.050(3) 0.048(3) -0.002(2) -0.002(2) -0.008(2) C6 0.038(3) 0.029(3) 0.037(3) 0.002(2) -0.015(3) -0.019(3) O6 0.030(2) 0.042(2) 0.061(3) -0.004(2) -0.020(2) -0.009(2) O7 0.070(3) 0.043(2) 0.062(3) -0.008(2) -0.028(3) -0.029(2) C7 0.037(3) 0.031(3) 0.033(3) -0.006(2) -0.005(3) -0.016(3) O8 0.092(4) 0.057(3) 0.032(2) 0.017(2) -0.029(2) -0.049(3) C8 0.050(4) 0.037(3) 0.033(3) -0.003(2) -0.013(3) -0.026(3) C11 0.028(3) 0.024(2) 0.026(3) 0.004(2) -0.010(2) -0.010(2) C12 0.037(3) 0.042(3) 0.025(3) -0.002(2) -0.001(2) -0.026(3) C13 0.045(4) 0.051(4) 0.038(3) -0.001(3) -0.006(3) -0.035(3) C14 0.041(3) 0.044(3) 0.040(3) -0.005(3) -0.017(3) -0.020(3) C15 0.044(4) 0.041(3) 0.027(3) -0.003(2) -0.012(3) -0.010(3) C16 0.031(3) 0.037(3) 0.025(3) -0.002(2) -0.002(2) -0.014(3) C21 0.026(3) 0.027(2) 0.023(2) 0.0004(19) -0.005(2) -0.015(2) C22 0.023(3) 0.033(3) 0.033(3) 0.001(2) -0.007(2) -0.007(2) C23 0.027(3) 0.044(3) 0.035(3) -0.004(3) -0.005(3) -0.008(3) C24 0.042(3) 0.046(3) 0.026(3) -0.001(2) -0.006(3) -0.021(3) C25 0.052(4) 0.037(3) 0.032(3) 0.011(2) -0.017(3) -0.021(3) C26 0.040(3) 0.030(3) 0.026(3) 0.003(2) -0.011(2) -0.010(3) C31 0.023(3) 0.028(3) 0.026(3) 0.000(2) -0.005(2) -0.011(2) C32 0.030(3) 0.031(3) 0.038(3) -0.006(2) -0.008(2) -0.011(2) C33 0.025(3) 0.048(4) 0.050(4) -0.005(3) -0.009(3) -0.016(3) C34 0.027(3) 0.046(4) 0.046(4) -0.007(3) -0.010(3) 0.001(3) C35 0.043(4) 0.026(3) 0.070(5) -0.006(3) -0.012(3) -0.006(3) C36 0.035(3) 0.031(3) 0.057(4) 0.001(3) -0.011(3) -0.015(3) C41 0.027(3) 0.029(3) 0.021(2) 0.0067(19) -0.007(2) -0.016(2) C42 0.028(3) 0.029(3) 0.033(3) 0.001(2) -0.010(2) -0.017(2) C43 0.029(3) 0.035(3) 0.019(2) 0.009(2) -0.010(2) -0.017(2) C44 0.031(3) 0.040(3) 0.042(3) -0.005(3) -0.008(3) -0.016(3) C45 0.027(3) 0.056(4) 0.049(4) -0.002(3) -0.010(3) -0.013(3) C46 0.028(3) 0.063(4) 0.045(4) 0.009(3) -0.015(3) -0.025(3) C47 0.039(3) 0.053(4) 0.039(3) 0.010(3) -0.015(3) -0.032(3) C48 0.030(3) 0.035(3) 0.029(3) 0.009(2) -0.014(2) -0.020(2) C49 0.047(4) 0.030(3) 0.042(3) 0.008(2) -0.018(3) -0.025(3) C50 0.034(3) 0.029(3) 0.036(3) 0.000(2) -0.011(3) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.929(5) . ? Re1 C2 1.944(5) . ? Re1 C3 1.986(5) . ? Re1 C4 1.997(5) . ? Re1 S1 2.4642(12) . ? Re1 Ag1 2.8199(9) . ? Re1 Re2 3.1077(8) . ? Re2 C7 1.927(5) . ? Re2 C8 1.949(6) . ? Re2 C5 1.974(6) . ? Re2 C6 1.996(6) . ? Re2 S1 2.4733(14) . ? Re2 Ag1 2.8476(6) . ? Ag1 P1 2.4483(14) . ? S1 C41 1.787(5) . ? P1 C11 1.816(5) . ? P1 C31 1.821(5) . ? P1 C21 1.824(5) . ? O1 C1 1.153(6) . ? O2 C2 1.152(6) . ? O3 C3 1.136(6) . ? C4 O4 1.130(6) . ? C5 O5 1.138(7) . ? C6 O6 1.135(7) . ? O7 C7 1.148(6) . ? O8 C8 1.149(6) . ? C11 C16 1.393(6) . ? C11 C12 1.404(6) . ? C12 C13 1.384(6) . ? C13 C14 1.378(7) . ? C14 C15 1.376(7) . ? C15 C16 1.375(7) . ? C21 C22 1.383(6) . ? C21 C26 1.398(6) . ? C22 C23 1.388(7) . ? C23 C24 1.381(7) . ? C24 C25 1.363(7) . ? C25 C26 1.386(7) . ? C31 C32 1.384(6) . ? C31 C36 1.384(6) . ? C32 C33 1.371(7) . ? C33 C34 1.378(7) . ? C34 C35 1.369(7) . ? C35 C36 1.377(7) . ? C41 C42 1.359(7) . ? C41 C50 1.416(7) . ? C42 C43 1.423(7) . ? C43 C44 1.408(7) . ? C43 C48 1.421(7) . ? C44 C45 1.361(8) . ? C45 C46 1.400(8) . ? C46 C47 1.359(9) . ? C47 C48 1.415(7) . ? C48 C49 1.408(8) . ? C49 C50 1.364(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 91.3(2) . . ? C1 Re1 C3 94.3(2) . . ? C2 Re1 C3 86.9(2) . . ? C1 Re1 C4 93.2(2) . . ? C2 Re1 C4 89.5(2) . . ? C3 Re1 C4 171.7(2) . . ? C1 Re1 S1 91.71(15) . . ? C2 Re1 S1 171.97(17) . . ? C3 Re1 S1 100.32(14) . . ? C4 Re1 S1 82.88(15) . . ? C1 Re1 Ag1 159.42(15) . . ? C2 Re1 Ag1 69.63(15) . . ? C3 Re1 Ag1 77.54(14) . . ? C4 Re1 Ag1 94.23(15) . . ? S1 Re1 Ag1 108.23(4) . . ? C1 Re1 Re2 142.10(14) . . ? C2 Re1 Re2 126.55(14) . . ? C3 Re1 Re2 86.70(14) . . ? C4 Re1 Re2 89.47(15) . . ? S1 Re1 Re2 51.12(3) . . ? Ag1 Re1 Re2 57.175(18) . . ? C7 Re2 C8 91.8(2) . . ? C7 Re2 C5 90.9(2) . . ? C8 Re2 C5 92.3(2) . . ? C7 Re2 C6 92.9(2) . . ? C8 Re2 C6 87.4(2) . . ? C5 Re2 C6 176.2(2) . . ? C7 Re2 S1 93.95(16) . . ? C8 Re2 S1 174.25(15) . . ? C5 Re2 S1 88.27(15) . . ? C6 Re2 S1 91.66(16) . . ? C7 Re2 Ag1 158.74(16) . . ? C8 Re2 Ag1 67.20(15) . . ? C5 Re2 Ag1 87.05(15) . . ? C6 Re2 Ag1 89.37(14) . . ? S1 Re2 Ag1 107.12(3) . . ? C7 Re2 Re1 144.82(16) . . ? C8 Re2 Re1 123.41(15) . . ? C5 Re2 Re1 88.37(15) . . ? C6 Re2 Re1 88.66(15) . . ? S1 Re2 Re1 50.86(3) . . ? Ag1 Re2 Re1 56.322(18) . . ? P1 Ag1 Re1 147.14(4) . . ? P1 Ag1 Re2 138.05(4) . . ? Re1 Ag1 Re2 66.50(2) . . ? C41 S1 Re1 116.87(17) . . ? C41 S1 Re2 109.64(16) . . ? Re1 S1 Re2 78.01(4) . . ? C11 P1 C31 103.2(2) . . ? C11 P1 C21 105.8(2) . . ? C31 P1 C21 106.7(2) . . ? C11 P1 Ag1 116.93(16) . . ? C31 P1 Ag1 106.13(15) . . ? C21 P1 Ag1 116.86(15) . . ? O1 C1 Re1 179.5(6) . . ? O2 C2 Re1 174.7(4) . . ? O3 C3 Re1 176.2(4) . . ? O4 C4 Re1 179.1(5) . . ? O5 C5 Re2 178.4(5) . . ? O6 C6 Re2 177.6(5) . . ? O7 C7 Re2 178.9(5) . . ? O8 C8 Re2 174.8(5) . . ? C16 C11 C12 118.5(5) . . ? C16 C11 P1 117.8(4) . . ? C12 C11 P1 123.6(4) . . ? C13 C12 C11 119.6(5) . . ? C14 C13 C12 120.5(5) . . ? C15 C14 C13 120.7(5) . . ? C16 C15 C14 119.3(5) . . ? C15 C16 C11 121.5(5) . . ? C22 C21 C26 118.9(5) . . ? C22 C21 P1 118.8(4) . . ? C26 C21 P1 122.3(4) . . ? C21 C22 C23 120.7(5) . . ? C24 C23 C22 119.8(5) . . ? C25 C24 C23 119.8(5) . . ? C24 C25 C26 121.3(5) . . ? C25 C26 C21 119.4(5) . . ? C32 C31 C36 118.2(5) . . ? C32 C31 P1 118.3(4) . . ? C36 C31 P1 123.4(4) . . ? C33 C32 C31 121.7(5) . . ? C32 C33 C34 119.8(5) . . ? C35 C34 C33 119.0(5) . . ? C34 C35 C36 121.6(5) . . ? C35 C36 C31 119.7(5) . . ? C42 C41 C50 119.9(5) . . ? C42 C41 S1 124.6(4) . . ? C50 C41 S1 115.5(4) . . ? C41 C42 C43 121.3(5) . . ? C44 C43 C48 119.0(5) . . ? C44 C43 C42 122.3(5) . . ? C48 C43 C42 118.7(5) . . ? C45 C44 C43 120.9(5) . . ? C44 C45 C46 120.4(6) . . ? C47 C46 C45 120.3(5) . . ? C46 C47 C48 121.2(5) . . ? C49 C48 C47 123.6(5) . . ? C49 C48 C43 118.2(5) . . ? C47 C48 C43 118.2(5) . . ? C50 C49 C48 122.1(5) . . ? C49 C50 C41 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.986 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.148 #=END